Six monocarboxylic acids were prepared highly enriched with 13C in their CO2H groups, and their pKa values were determined at low concentrations 10− 4− 10− 5M in H2O and in H2O-(CD3) 2SO mixtures by analysis of pH-dependent 13CO2H NMR chemical shifts. Plots of the variation of CO2H (CO2−) 13C-NMR chemical shift vs pH gave a typical titration curve from which pKa's for [1-13C]-phenylpropionic (1) and [1-13C]-phenylacetic (2) acids were ...